Potassium Carbonate → HCID 58098809、化合物

HRID 533464

反応式

HRID 533464 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH:11][C:12](=[O:14])[CH3:13].[H-].[Na+].C([O-])([O-])=O.[K+].[K+].Cl.Cl[CH2:25][CH2:26][N:27]1[CH2:31][CH2:30][CH2:29][CH2:28]1>CN(C=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([O:1][CH2:25][CH2:26][N:27]2[CH2:31][CH2:30][CH2:29][CH2:28]2)=[C:3]([NH:11][C:12](=[O:14])[CH3:13])[CH:4]=1)([O-:10])=[O:9]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 816681-(2-Chloroethyl)pyrrolidine hydrochlorideHCID 3292867Acetamide, N-(2-hydroxy-5-nitrophenyl)-

生成物 1

HCID 58098809HCID 58098809、化合物収率 33%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of N-(2-hydroxy-5-nitrophenyl)acetamide (870 mg, 4.44 mmol) in DMF (5 mL) was added NaH (196 mg, 5.32 mmol) and K2CO3 (2.11 g, 13.32 mmol), followed by 1-(2-chloroethyl)pyrrolidine hydrochloride (905 mg, 5.32 mmol). After heating at 100° C. for 20h, the solution was poured to ice, and was extracted with EtOAc, organic layer was washed with Sat. NaHCO3, brine, dried and concentrated to give N-(5-nitro-2-(2-(pyrrolidin-1-yl)ethoxy)phenyl)acetamide (430 mg).

後処理

  1. additionthe solution was poured to ice
  2. extractionwas extracted with EtOAc, organic layer
  3. washwas washed with Sat. NaHCO3, brine
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8d1a65f1c54b4bc6b776dfccd7943cc4
出典データセット
uspto-grants-2014_10
特許番号
US08853230B2

関連ノート

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